Browsing by Subject "Human tissues"

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    Open Access
    Evaluation of distribution of emerging mycotoxins in human tissues: applications of dispersive liquid–liquid microextraction and liquid chromatography‑mass spectrometry
    (Springer, 2023-11-21) Castell Martínez, Ana; Arroyo Manzanares, Natalia; Palma Manrique, Rosa; Campillo Seva, Natalia; Torres, Carmen; Fenoll, José; Viñas López-Pelegrin, Pilar; Química Analítica
    In this work, a complete study of the distribution of emerging mycotoxins in the human body has been carried out. Specifically, the presence of enniatins (A, A1, B, B1) and beauvericin has been monitored in brain, lung, kidney, fat, liver, and heart samples. A unique methodology based on solid–liquid extraction (SLE) followed by dispersive liquid–liquid microextraction (DLLME) was proposed for the six different matrices. Mycotoxin isolation was performed by adding ultrapure water, acetonitrile, and sodium chloride to the tissue sample for SLE, while the DLLME step was performed using chloroform as extraction solvent. Subsequently, the analysis was carried out by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC–MS/MS). The proposed method allowed limits of quantification (LOQs) to be obtained in a range of 0.001–0.150 ng/g, depending on the tissue and mycotoxin. The precision was investigated intraday and interday, not exceeding of 9.8% of relative standard deviation. In addition, trueness studies achieved 75 to 115% at a mycotoxin concentration of 25 ng/g and from 82 to 118% at 5 ng/g. The application of this methodology to 26 forensic autopsies demonstrated the bioaccumulation of emerging mycotoxins in the human body since all mycotoxins were detected in tissues. Enniatin B (ENNB) showed a high occurrence, being detected in 100% of liver (7 ± 13 ng/g) and fat samples (0.2 ± 0.8 ng/g). The lung had a high incidence of all emerging mycotoxins at low concentrations, while ENNB, ENNB1, and ENNA1 were not quantifiable in heart samples. Co-occurrence of mycotoxins was also investigated, and statistical tests were applied to evaluate the distribution of these mycotoxins in the human body.
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    Monitoring of hydroxylated polycyclic aromatic hydrocarbons in human tissues: targeted and untargeted approaches using liquid chromatography‐high resolution mass spectrometry
    (Wiley-VCH Verlag , 2023-07-04) León Morán, Lixy Olinda; Pastor Belda, Marta; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Torres Sánchez, Carmen; Viñas López-Pelegrin, Pilar; Química Analítica; Facultades de la UMU::Facultad de Química
    Hydroxylated polycyclic aromatic hydrocarbons are metabolites of persistent organic pollutants which are formed during the bioactivation process of biological matrices and whose toxicity is being studied. The aim of this work was the development of a novel analytical method for the determination of these metabolites in human tissues, known to have bioaccumulated their parent compounds. Samples were treated by salting‐out assisted liquid‐liquid extraction and the extracts were analyzed by ultra‐high performance liquid chromatography coupled to mass spectrometry with a hybrid quadrupole‐time‐of‐flight analyzer. The proposed method achieved limits of detection in the 0.15–9.0 ng/g range for the five target analytes (1‐hydroxynaphthalene, 1‐hydroxypyrene, 2‐hydroxynaphthalene, 7‐hydroxybenzo[a]pyrene, and 9‐hydroxyphenanthrene). The quantification was achieved by matrix‐matched calibration using 2,2´‐biphenol as internal standard. For all compounds, relative standard deviation, calculated for six successive analyses, was below 12.1%, demonstrating good precision for the developed method. None of the target compounds was detected in the 34 studied samples. Moreover, an untargeted approach was applied to study the presence of other metabolites in the samples, as well as their conjugated forms and related compounds. For this objective, a homemade mass spectrometry database covering 81 compounds was created and none of them was detected in the samples.